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Vialaysiaig : Guidelines on Food Sampling PART 1: GENERAL PRINCIPLES AND PROCEDURE art Ls General Pimples And Ps FOREWORD Since 1974, the activities carried out by the Food Quality Control Unit, Ministry of Health had expanded tremendously due to increased awareness of food safety by the publie and the rapid growth of food industry in the country. The Food Act 1983 and the Food Regulations 1985 are being continuously being legislated to help ensure that the public in Malaysia are consuming safe and quality food. One of the main activities in the Food Quality Control programme is Food Sampling. Proper food sampling in an overall food inspection programme is very important because suspect foods for either legal or monitoring purposes should be properly obtained to get accurate results. It is for this reason that the Food Quality Control Division of the Ministry of Health had initiated a Working Group to prepare a “Malaysian Guidelines on Food Sampling”. This Guideline on Food Sampling is subject to periodical review to keep abreast of the latest developments. Suggestions for improvements will be recorded and in due course brought to the notice of the Working Group, Ministry of Health of Malaysia would like to congratulate and gratefully acknowledges the valuable contributions of all the following :~ Dr. Tee E Siong Institute for Medical Research (Chairman) Cik Faridah Mohd. Som Malaysian Agricultural Research and Development Institute, Food Technology Centre Puan Radziah Mohd. Daud Standard and Industrial Research Institute of Malaysia Encik N.H. Jeevan Chemistry Department Puan Aini FawziaSamsudin Chemistry Department Dr. Mohd. Yazid Manap Universiti Pertanian Malaysia, Faculty of Food Science and Biotechnology Tuan Syed Zainal Abidin Ministry of Housing and Local Government, Bin Syed Harun Department of Local Government Encik Mohd. Zainuldin Taib _ Institute for Medical Research Encik Rashidi bin Hasbullah Ministry of Health, Selangor Health Department Encik Thayalan Ramadas Ministry of Health, Selangor Food Quality Control Laboratory Encik Ho Nee Yong Ministry of Health, Penang Health Department ‘Tuan Hj. Zulkifli Abdul Ministry of Health, Health Inspectorate Rahman Dr, Mustafa Bakri Adnan Ministry of Health, Food Quality Control Division Pest 1 General Rrincpien And Procedure Puan Norrani Eksan Ministry of Health, Food Quality Control Division Encik Louis Lee Yoon Sin Ministry of Health, Food Quality Control Division Encik Jamal Khair bin Hashim Ministry of Health, Food Quality Control Division Puan Noraini Dato’ Ministry of Health, Food Quality Control Division Mohd. Othman (Secretary until 1 November 1995) Mariam Abdul Latif Ministry of Health, Food Quality Control Division (Secretary until 1 November 1995) This is a general guideline to be used as a reference by state level enforcement teams and the laboratory staff. ‘This working Group has worked very hard to prepare this Guideline and I would like to express my gratitude and thank every one of them for their contribution and cooperation. Deputy Director General (Public Health), Ministry of Health Malaysia, ‘August 1996 oth 1: General Principay And Procedere SECTION 1. INTRODUCTION ‘The series of Malaysian Guidelines on Food Sampling are designed to ensure that fair and valid sampling procedures are used when food is tested for compliance with the Food Act 1983 and the Food Regulations 1985. The sampling methods are intended for use as standardized methods designed to avoid or remove difficulties which may be created by diverging legal, administrative and techinical approaches to sampling and by diverging interpretation of results of analysis in relation to lots or consignment of foods. ‘The authorized officer should remember that the reliability of the laboratory's results can only be as good as the sample submitted. Mistakes such as not collecting sufficient sample or deficiencies in collecting the sample such as contamination by authorized officer affect the laboratory's findings. The submitted sample may be the only basis for rejecting a shipment of food from entry into the country, removal of a product from the marketplace, or some other legal or administrative action which may have adverse effects to the manufacturers and traders. Improperly sampled food may also result in dangerous products remaining on the market with potential adverse consequences to the customer. Proper sampling techniques must be used by the authorized officer to assure that the sample analyzed by the laboratory reflects the conditions existing in the lot of food at the time the sample was collected. This present Malaysian Guideline on Food Sampling Part 1: General Principles and Procedures is intended to provide guidelines for the collection of food samples. It ean be used as a reference for state level enforcement and laboratories preparing more detailed working protocols to produce manuals for their use. It provides sufficient information for the collection of samples in most situations encountered by the authorized officer as defined under the Food Act 1983, but the details of method of sampling for contaminants and multitude of food products would be elaborated further under other volumes of this series of the Malaysian Guidelines on Food Sampling. In preparation of this guideline on sampling, various international publications were referred to (see Reference). SECTION 2. DEFINITIONS 24 22 23 24 25 26 Acceptable Quality Level (AQL) One of the initial consideration in the development of a statistical acceptance sampling plan is the selection of an appropriate AQL or Acceptable Quality Level. This characteristic is defined as the maximum percent defective units in lots that will be accepted most of the time (approximately 95 percent of the time). Lats or production unit with more defective material will be accepted less oftent ~ the ratio of rejection to acceptance will increase as the sample size increases. Any value of AQL which is selected must be one which is realizable, in practice, and ‘economically viable, ‘Acceptance Number (¢ ) Foragiven attribute sampling plan, the maximum number of defective items (or of defects) allowed in the sample that permits acceptance of the lot. Attribute See Characteristic Batch Units of the same product manufactured at the same time under the same conditions so that they will be about the same quality, Packages of these units would normally bear a batch number that identifies the production during a particular time interval, and usually ftom a particular ‘line’, retort, or other critical processing unit. Bulk Container As defined under Regulation 2 (1) of the Food Regulation 1985 “bulk container” includes - (@) any wagon, crate, silo, tanker and other similar container; and (b) any box, carton and other similar container in which more than one duly labelled package and its content are placed and in which the packages and their contents are not intended to be retained when the packages or the contents are sald by way of retail. Bulk Sample (2) collection of increments or groups thereof intended taken from a bulk container (raw bulk sample). (2) composite of the increments taken from a bulk container (bulk sample in a proper sense). (3) Acombined aggregation of the items or portions of items taken from a lot of prepacked products (bulk sample). 27 28 29 240 2m 242 243 2.14 245 Characteristic A property which helps to differentiate between the items of a given lot into acceptable and un- acceptable items. The differentiation may be either quantitative (by variables) or qualitative (by attributes). Complainant Sample One or more items or increments which may not provide information representative of the po- pulation (lot or consignment). See Sample. Cluster Sampling ‘A method of sampling in which the tot is divided into aggregates (or clusters) of items bound to- gether in some manner. A sample of these clusters is taken at random and all items within a clus- ter are included in the sample. Composite Sample ‘A sample consisting of portions from each unit, taken in proportion to the quantity in each unit selected. Consignment ‘A quantity of the same commodity delivered at one time and covered by one set of documents. The consignment may consist of one or more lots or parts of lots. Consumer's Risk (CR) The probability that a lot will be accepted on the basis of results of test samples when in reality the lot as a whole is substandard relative to the stated criteria of acceptability. Note: The probability acceptance will depend on the severity of defects. Continuous Sampling ‘Sampling inspection by attributes applied to a continuous flow of individual units of products (see /tem) that (a) _ involves acceptance and rejection on a unit by unit basi (b) employs altemate periods of 100% inspection and sampling, depending on the quality of submitted product. Defective Not suitable for the intended purpose. Defective Item An item containing one or more defects. 2.16 247 2.18 2.19 2.20 Post 1: General Priniplay Aad Prose Note: - Defect means a failure of a unit to meet one or more of the specified requirements, In the order of significance of the specifications, defects can often be classified as follows: (@) Critical Defect: A defect that, according to judgement and experience, is likely to result in hazardous or unsafe conditions for individuals using, maintaining or depending upon the product, or that is likely to prevent performance of the function of a major product. (b) Major Defect: A defect other than critical, that is likely to result in a failure or to reduce materially the usability of the product for its intended purpose. (©) Minor Defect: A defect that is not likely to reduce materially the usability of the product for its intended purpose or that is a departure from established specifications having little bearing on the effective use or operation of this product. Homogeneity and heterogeneity ‘The degree to which a property of a substance (the observed values of a characteristic) is uniformly distributed throughout a quantity of material (a lot). Ina statistical sense, a lot should be considered homogeneous in relation to a given characteristic ifits distribution is assessed to be approximately normal and its standard deviatioa fow. On the contrary, when this distribution is far from normal (for example bimodal) and/or the relevant standard deviation is high, the lot should be considered heterogeneous. Note: - Items in a lot may have homogeneous distribution of one characteristic and simultaneously a heterogeneous distribution of another. Increment A quantity of material taken at one time from a larger body of material. Note: - Increments may be tested individually aiming at estimation of the variation of any cha- acteristic throughout a lot (or between lots). See also Bulk Sample. Individual See Item Inspection ‘The process of examining, measuring, testing, gauging or otherwise comparing the unit with applicable requirements. Inspection by Attributes, A method which consists in taking note, for every item of a lot or of a sample taken from this lot, of the presence or absence of a certain qualitative characteristic (attribute) and in counting how ‘many items have or do not have this characteristic. Detailed methodology can be found in ISO 2859. 2.21 2.22 2.23 2.24 2.25 2.26 227 2.28 2.28 2.30 2.31 Inspection by variables ‘A method which consists in measuring a quantitative characteristic (variable) for each item of a Jot or of a sample taken from this lot. Details of the method are Given in ISO 3951. Inspection Level ‘The term used to indicate the relative amount of sampling performed on lots of a product or class of products. ttem A defined quantity of a product on whieh a set of observations may be made. Laboratory Sample A sample as prepared for sending to the laboratory and intended for inspection or testing, Limiting Quantity Level: See Rejectable Quality Level Lot collection of units of a product from which a sample is to be drawn to determine acceptability of the product. Note: - A lot may consist of one or more batches. A lot could also be a consignment or shipment to one destination. Lot Size ‘The number of items or quantity of a product constituting the lot. Mean In ordinary usage, the arithmetic mean; i. the sum of 1 number of observations divided by 7. See Variance. Multiple Sampling Sampling inspection in which sets of replicate items up to a specified sum are taken. After examining one set, a decision can be made to accept the lot, to reject itor to examine another set. Subsequent decisions are based on an increasing sum of items, associated with decreasing rate of growth of acceptance number. Having inspected the last set, a decision to accept or reject the lot must be reached. Multi-Stage Sampling A type of sampling in which a sample is selected by stages, the sampling units at each stage being subsampled from larger units chosen at the previous stage, Nested Sampling : See Multi-Stage Sampling 2.32 2.33 2.34 2.35 2.36 2.37 2.38 2.39 2.40 244 Pant 1: General Priniplan And Procedure [Normal Distribution: The density function for a normal random variable, ys {a fv-x) ve sin Tae | ( > P OOK YK +00 where wand gare the two parameters of the normal distribution with mean and variance Operating Characteristic Curve (0C-Curv Acurve showing, for a given sampling plan, the probability of acceptance of alot as a function of its actual quality. Package As defined under Part 1 Section 2 of the Food Act 1983, “package” includes anything in which or any means by which food is wholly or partly cased, covered, enclosed, contained, placed or other- ‘wise packed in any way whatsoever and includes any basket, pail, tray or receptacle of any kind whether opened or closed. Packat ‘The art of and the operations involved in the preparation of articles or commodities for carriage, storage and delivery. Pe iodic Sampling: See Systematic Sampling Primary Sample ‘A sample taken from a lot during the first stage of multi-stage sampling, Note: - Accordingly, the sample taken from the primary sample is called the secondary sample, ete. The final sample is taken during the last stage. Probability of Acceptance The likelihood that a lot of known quality would be accepted on the basis of results of test samples relative to the stated criteria. Probability of Rejection The likelihood that a lot of a given quality will be rejected by a given sampling plan. Producer's Risk (PR) ‘The probability that a lot of acceptable quality will be rejected on the basis of results of test samples relative to the stated criteria of acceptability Quality Inspection: See Quality Control. 2.42 2.43 2.44 2.45 2.46 2.47 2.48 Quality Controt The set of operations intended to maintain or to improve quality. Random Sampling The taking of 7 items from a lot of Witems in such a way that every sample of size 7 has an equal chance of selection, hence excluding bias. A table of random numbers may be used. Reduce Sample A sample obtained from a bulk sample by reducing its quantity without change of composition. Notes: - 1) It may also be necessary to reduce the particle size in the course of reducing the quantity. 2) Usually, most laboratory samples, reference samples, and storage samples (i.e. the so-called “final samples” in the traditional meaning of the term) can be prepared in this way. Reference Sample ‘A sample prepared at the same time, and having the same properties, as the laboratory sample, and which is acceptable to the parties concerned and retained for use as laboratory sample if a disagreement oceurs. Rejectable Quality Level (RQL) Quality ofa lot expressed as the percentage of defective items (or defects per hundred units) in the lot which is considered to be unacceptable as a process average in continuous production and is associated with a low probability of acceptance (usually in the region of 10%). ‘Note: - This quality level may correspond to the critical number of defectives observed in sampling inspection (i.e. lot tolerance percent defective) or to a mean of a variable to which the actual ‘mean is compared. Representative Sample A sample drawa so as to reflect as accurately as possible the properties of interest of the lot (the bias of the sample should be a minimum against the lot) from which it is taken. Sample ‘One or more items or increments selected (ideally at random) from a population (lot or consign ‘ment) intended to provide information representative of the population (lot or consignment). It may serve as a basis for a decision on the population or on the process which had produced it. Note:- Food item brought to the attention of health authorities by complainant, sometimes refered to as“ sample”, cannot provide information representative of the population (lot or consignment) and hence cannot be considered as sample under this definition. See Complainant Sample. 1 And Procedere ic 2.49 Sample Size ‘The number of items or quantity of a products constituting the sample, drawn from a lot or production. 2.50 Sampling ‘The process of drawing or selecting items or quantity of a product from a lot or produ 2.51 Sampling Error That part of total estimation of error of a characteristic due to the heterogeneity of the characters, the random nature of sampling and to known and acceptable deficiencies in the sampling plan. 2.52. Sampling Plan ‘The predetermined procedure for the selection, withdrawal and preparation of samples from a ot and acceptance and or rejection criteria to serve as the basis for a decision as to the acceptance or rejection of the lot. 2.53. Simple Random Sampling: See Random Sampling. 2.54 Sequential Sampling ‘A method of sampling which consists in taking successive items, or sometimes successive group of items, but without fixing their number in advance, the decision to accept or to reject the lot being taken as soon as the cumulative result permits action, according to rules laid down in advance. 2.85 Standard Deviation ‘The positive square root of the Variance (see Variance). 2.56. Stratified Random Sampling ‘The sampling of a lot which can be differentiated into sublots (called strata or zones), in such a way that specified proportions of the sample are drawn at random from the different strata. 2.87 ‘A technique for dividing consignments into logical groupings such as size of cans, grades, box, eases, which controls known sources of variation. It may be used where prior knowledge exists that the consignment is not homogenous. 2.58 Systematic Sampling A method of sampling which consist of taking at a fixed interval that will provide the desired number of items. 2.59 2.60 261 2.82 2.63 Test Sample Asample prepared from the laboratory sample according to the procedure specified in the method of test and from which test portions will be taken. Vari ‘The differences in an observed characteristic throughout the lot. Variable See Characteristic. Variance A measure of dispersion based on the mean squared deviation from the arithmetic mean. Zone Sampling: See Stratified Random Sampling, Fort 1: Ganaral Principles And Procedure SECTION 3. PRINCIPLES OF SAMPLING 34 Definition and Objective of Sampling A sample may be defined as one or more items or increments selected (ideally at random) from a population (lot or consignment) intended to provide information representative of the population (tot or consignment). It may serve as a basis for decision on the popula- dion or as the process on the population or as the process which had produced it. Since most foods to be sampled are not homogenous in their makeup or in suspected adultera- tion, collection of a perfect sample is often not possible. The objective of sampling is to select a certain portion, number of containers, or product units that is most representative of a consignment or lot of food from which it is collected, The sample size should be suf- ficient to allow laboratory analysis and repeat analysis, if necessary. ‘The condition of the sample should reflect conditions at the time the product was sam- pled. For example: ~ a sample containing or suspected of containing live insects should be fumigated so that insects are killed and to prevent an increase in the number of such insects in the sample between the time of collection and the time of laboratory analysis, - _asample should not be exposed to extreme temperatures that could change the pro- duct and thus affect the outcome of the planned analysis. It is important to synchronize inspection and laboratory priorities to ensure that samples from an inspection will be promptly analyzed. It may not be necessary to have samples analyzed when there is strong evidence that laboratory results will confirm the inspect- ional observations. However, if prosecution, seizure, embargo or some other type of for- mal legal action is indicated there may be a need for analytical support. For example, the authorized officer’s observation and documentation of insects or rodent exereta in or around a lot of food is evidence for which the authorized officer can testify. However, if more precise information is needed about the species of insect or type of rodent suspected of causing the adulteration the sampte should be submitted for analysis even if the intended action is administrative rather than legal. The final objectives of every sampling should be clearly defined ahead of time. The labo- ratory capability, methods of analysis and amount of sample must be determined and the sampling methods and techniques considered before the sample is actually collected. In some cases and situations where samples are sent directly to a designated laboratory for testing, the laboratory results may not be available until after the product has moved into consumer markets and become untraceable. Because of this pragmatic limitation, some food containing violative residues may inevitably pass into consumer markets, regardless of the regulatory control efforts to limit this occurrence as much as possible. However if a food is found to be adulterated or in violation of the law, action could still be taken against the firm. A mechanism must be in place to recall food from the market. The firm should be blacklisted for further consignments of food. 32 324 iples And Proce Types of Sampling Selective Sampling In selective sampling, samples are normally collected either to illustrate or document unsatisfactory conditions observed by the authorized officer, or to provide for laboratory analysis a unit of food suspected of being adulterated. It is designed to investigate and control the movement of potentially adulterated products. Sampling can be performed at any point in the food chain, during an inspection, at a warehouse or wholesaler or at the market or retail level. Samples collected as a result of a consumer complaint, inspectional observations or other type of lead are generally “selected”, that is, they are selected in a ‘manner that affords the best opportunity to confirm certain known facts. Normally, the proper drawing ofa representative sample from a given food lot would be conducted in such a way that the bias of the authorized officer or sampler would not play arole. However, when sampling for the regulatory purposes the goal of selecting a totally representative sample is not considered because the authorized officer interest is in incre- asing the probability of detecting defective products. Some examples are: Example 1 The authorized officer observes an employee dumping a raw material into a hopper from a'bag with rodent exereta pellets adhering to the outer surface. He/she suspects the pellets may have become a part of the food being manufactured. The authorized officer therefore selects a sample of the product bearing the code being used at the time of the observation. Example 2 A consumer complaint of insects in a manufactured food product received. Since the consumer package has been opened the authorized officer cannot determine where the adulteration took place. As an initial step the authorized officer selectively samples from the same lot from which the complainant product was purchased. Example 3 During a warehouse inspection rodent entryways are noted on the outside of the building and confirmed by the finding of fresh rodent excreta pellets inside of the building near the opening. The authorized officers examines a lot of food stored near the rodent entryway and selectively samples from containers showing suspect- cd rodent urine stains when examined under ultraviolet light. Selective sampling procedures are used to increase the possibility of locating sub- standard or defective products. As indicated in the above examples inspectional observations or some other lead dictates the need for selective sampling. Example 1 employs both selective and objective sampling techniques. The authorized officer selects a suspect code within a lot of food to sample but then uses an objective sampling method within that code unless the inspectional evidence is even more container specific. Different kinds of administrative procedures may be used to try to correct a firm’s violative practices before legal action is initiated. Such administrative actions sometimes require an official or group of officials to make a decision on what to do about such firms. The more evidence provided to these officials the easier itis for them to make a decision in favour of the consumer. Selective sampling is a method that stands the best chance of providing such information. 13 lat And Procedure 322 The sampling is often purposely biased and is directed at particular products or producers in response to information from stastistically based sampling (or other regulatory control agency data), or from observation of authorized officer during inspection indicating that violations may be present. On site testing procedures may be performed by the authori- zed officer, or samples may be submitted for analysis to a laboratory. Depending upon the weight of evidence for testing in support of selective sampling, product may be retained until test results indicate the appropriate regulatory disposition. Laboratory analysis of selected test samples should be completed as rapidly as possible and take precedence over routine, stastistically based samples. In selective sampling situations, lots should be considered unacceptable until it can be demonstrated that they are in compliance with the Food Regulations 1985 or national regulations of the country importing the food. Failing to detect a violation, different sample sizes and prevalence of violation frequen- cy can be determined as showa in the following example with reference to Appendix | In selecting 5 samples from a large lot in which 10 percent of the units has 10% violation would, on the average, fail to detect a residue violation in 59.0 percent of such lots (i.e., 59.0 percent of the lots would be accepted). Assuming the same conditions as the previ- ous example, but using a sample size of 50, would result in only 0.5 percent of such lots being accepted. Objective Sampling In objective (non-biased) sampling, the samples are most often collected from a lot of food on a routine basis for surveillance, for collection of data for a specific purpose, or for monitoring to determine whether the food is unsatisfactory for any reason. This may be done where inspections do not show unsatisfactory conditions or when inspections cannot be made frequently. Objective sampling is designed to provide profile information. The focus is on gathering information on the incidence of violations; therefore, only characteristic with established safe limits are considered for testing programs, Characteristics selected for statistically designed non-biased sampling are usually based on risk profiles and the availability of laboratory methods suitable for regulatory control purposes. Information is obtained through a statistically based selection of random samples. Limited or geographical area sampling may be conducted where a localized potential problem appears. The informa- tion obtained from this type of sampling should be reviewed periodically to assess con- trol programs and to allocate resources according to specific needs. In addition to profile information, data provides a basis for further regulatory action, In particular, the results can be used to identify producers marketing a food commodity with violative concentrations. These producers subsequently will be subjected to more directed and specific sampling and testing until compliance is demonstrated. Other auxiliary uses of the data are to indicate prevalence and concentrations of violations, to other corrective efforts may be needed. Thus, objective sampling gathers information and assists in deter- ring practices that lead to violations Objective samples generally are collected in the market place but may also be collected in the possession of the manufacturer. Objective sampling is the method most used for imported food products because the manufacturing operations of the exporting country firm cannot be observed, thus no leads are provided for the collection of selective samples. | Past 1 3.23 As a general practice, samples collected by authorized officer are sent for analysis to la boratories designated by government. However, samples may also be sent to other labo- ratories for general and specific analysis. In these situations, the authorized officer may send samples to a laboratory designated by national authorities for more definitive ana- lysis when results obtained from the screening test suggest a positive finding. In some cases and situations where samples are sent directly to a designated laboratory for testing, the laboratory results may not be available until after the product has moved into consumer markets and become untraceable. Because of this pragmatic limitation, some food containing violative residues may inevitably pass into consumer markets, regardless of the regulatory control efforts to limits this occurrence as much as possible. The consequences to public health, however, are minimal as long as the frequency of violations is low. Determination of Sample Size 3.23.1 Selective Sampling In selective sampling it is recommended that at least 6 and usually no more than 30 primary samples be analyzed from a suspect lot. The smaller number of samples would be appropriate, for example, when the suspected contami- nation is likely to occur throughout the lot, or when the location of probable contamination (e.g., surface contamination) is readily identified. Table | provides statistical information that may be helpful in deciding the number of samples to be analyzed in a particular case. International harmony in control procedures is not dependent on the number of primary samples analyzed be- cause the criteria for acceptance is applied to each primary sample. However as shown in Table 1, the larger the number of samples taken, the greater the assurance that products not in compliance will be detected. Table 1 is used based on confidence level and incidence rate. For example, if violation incidence is estimated at 10%, confidence of 95%, then the minimum samples required is 29 with the known violation rate, TABLE 1 ATTRIBUTE PLAN TO DETECT INCIDENCE RATE IN A POPULATION NUMBER OF SAMPLES REQUIRED TO DETECT AT LEAST ONE VIOLATION WITH PREDEFINED PROBABILITIES (I.E., 90, 95 AND 99 PERCENT) IN A POPULATION HAVING A KNOWN VIOLATION INCIDENCE RATE Violation Incidence Minignum number of samples (n,) required (9) ma Population to dotect a violation witha confidence of 90% 95% 999 35 6 7 a 30 7 9 B 2s 9 1 v 20 in 4 2 13 15 19 29 10 2 29 44 5 6 59 0 1 230 299 459 5 460 598 9i9 1 B02 2995 4603 loop 2303ip 2.996!p 4.605ip 1c 3.2.3.2 * The number of primary samples does not depend on population size, except when the number of samples shown in the table is greater than about 10% of the population size, The following formula can be used to adjust the table values for the minimum number of primary samples (n,) and compute the required minimum number of primary samples (n)for a given lot size (N):! n=. 1+(,- 1) /N Objective Sampling Where no specific instructions are provided a general rule which may be followed is to colfect samples from the square root of the number of units in the lot to be sampled. For example let us assume that Figure | represents a lot of 36 cases, each case containing 36/0.5 kg packages of a food product, Applying the square root principle the authorized officer first determines that the square root of 36 is 6. This means that samples should be collected from 6 of the 36 cases. t\2X ie Xe NS 5 ° 7 Na ri} oe | 0) | ve 25 ASSTiISaSSSESISISALIIGIITTE —_| NED 29 21) 22 23 24 \\ 33 \ 33 | 34 35 | 36 Figure 1 For can products, some guidelines for selecting sample size has been established. The following Table can be used as a guide. ‘Table 2: Sample Size for Can Products Can-size Minimum number of samples 108 mm diameter x 123.8 mm height and smaller: small lots 24 cans up to 1000 cases 48 cans, each can from a different case 1001 to 3600 cases mye mom mm art 1: General Principles Aad Procedure larger cans: up to 600 cases 24 cans, each can from a different case 601 to 900 cases 30 cans, each can from a different case 901 to 1300 cases 36 cans, each can from a different case Source: FAO Food And Nutrition Paper 14, 1988. Reference number 2. 3.24 Method of Selecting Cases 3244 iii, iv, Simple Random Sampling Drawing a sample in such a way that every part of the lot has an equal chance of being represented is known as random sampling. Different methods may used to randomly select the six cases. One method is to place individually numbered slips from one to 36 in.a box, shake and withdraw one slip of paper, recording the number, returning the slip to the box, shake and repeat the procedure until six different numbers have been selected. This is considered random because each slip of paper has an equal chance of being selected. This is true only if after each drawing the slip is returned to the box. Othe odds would chan; r slip is withheld from consideration. Asamatter of practicality, however, most sampling situations are not conducive to using a formalized procedure as described above. The authorized officer may be in a freezer, on a hot loading dock or in the corner of some dimly lit warehouse. It, therefore, serves the sante purpose if the authorized officer se- lected six cases at random from throughout the lot making sure that each layer and all layers of a pallet load or stacks of products and that all areas are repre- sented, The authorized officer may decide to just randomly select every 5*or 6" cases from the lot. This may be the best method for the existing situation. Another method is to use random tables. To use a table of random numbers or digits, first give consecutive numbers to the packages, containers, or other units in the lot that is to be sampled, in any convenient order. Then pick a page of the table of random numbers (Appendix 2) — for example, by using numbered cards in a box. Next, without looking, bring a pencil point down on some place on the page. The digit nearest the point is the first digit of the number of the first sample package. Take as many columns to the right of that in which this digit appears as are needed to number all the packages in the lot. The digits in these columns in the same row as the first digit chosen complete the numtber of the first sample, The numbers of additional sample packages are the following nusnbers in the designated columns. Note that the colurn numbers are indicated at the top of the table and that each columns are arranged in groups of five to facilitate identification. For practical purpose — scientific calculator with random number can also be used to generate the required numbers. 9 Poet ts Ganerl Principles And 3.24.2 3.24.3 Stratified random sampling Samples are obtained by separating the population elements into some non overlapping groups, called strata, and selecting samples within each stratum according to a simple random design. Example of stratification are by countries, geographic regions and time. Tables of random numbers or equivalent proce- dures may be used to ensure randomization. ‘Systematic sampling Systematic sampling is a method of sampling which consist of taking at interval that will provide the desired number of units. An example of systematic samp- ling is taking a sample from every “X’ kilos of products imported from 2 par- ticular country. This method is convenient when there is reliable information on product volumes that can be used to determine the sampling interval that give the desired number of samples per month of year. Alternatively, samples may be systematically taken by time or number of shipments. As systematic sampling can be vulnerable to abuse if the system is predictable, itis advisable to build some randomness into the sampling interval 3.3 Sampling Plans ‘Sampling plan is defined as the predetermined procedure for the selection withdrawal and preparation of samples from a lot and acceptance and or rejection criteria to serve as the basis for a decision as to the acceptance or rejection a the fot. Sampling plans embrace all aspects of lot acceptance, 3.3.4 Types of Sampling Plans . 3344 @ i) Attribute Acceptance Sampling Plans. Sampling by attributes is sampling whereby either the item or the products is classified as defective or non-defective with respect to a given requirement or set of requirements. ‘The number of defective items, c, permitted in sample, is determined as follows: Determine the number of items to be inspected from lots Three inspection level I, II and III are given in Appendix 3 for general use. Generally, level II shall be used, Level I may be used when less discrimination is needed or level III when greater discrimination is required. Examples of use of switching between inspection levels are given in Appendix 4. ‘Two special level, S-3 and S-4 are also given in Appendix 3 and may be used where relatively small sizes are necessary and large sampling risk can or shall be tolerated e.g, For monitoring purpos Determine AQL to be used ii) 3342 3.34.3 Fart 1s Ganeral Select an AQL to be used depending on the characteristics i.e. low AQL (0.1% or 1.0%) for these characteristics which may be “health-risk” associated and higher AQL (6.5% or 10%) for compositional charateristics such as fat, moisture etc. Determine the acceptance number The lot is accepted when the number of defective items equals or less than the acceptance number (c). See Appendix 5. Variables Acceptance Sampling Plans for Mean Quality Sampling by variables is sampling whereby the values of a specified criterion for a set of items forming the sample are measured on a continuous scale and the values used to determine the acceptability or otherwise of the lot from which the items are taken e.g. determination of protein leve! or contaminant level in food. ‘The mean value of a characteristic X, is determined by the following steps: (i) Determine the number of items inspected from the lot Three inspection levels I, II and IIT are given in Appendix 6 for general use. Generally, level II shall be used. Level I may be used when less discrimination is needed or level III when greater discrimination is required. Examples of use of switching between inspection levels are given in Appendix 4. Two special levels, S-3 and S-4 are also given in Appendix 6 and may be used where relatively small sizes are necessary and large sampling risk can or shall be tolerated e.g. for monitoring purposes, di) Accept lot based on mean The lot is accepted when: q + Ultraviolet lamp + Stop watch + Glue * Magnifying glass. + Paint brush + Tweezers * Dry borer tube (for sampling flour, dried milk and dried milk products usually multi: walled paper bags. The sampled product generally will have to be push- ed out of the trier into a sample container with a spatula or a clean spoon. This particular trier should not be used for bacteriological sampling). + Sampling probe (for sampling railcar and lorryloads of dried grains such as wheat and maize). + Conical-shaped metal bag probe, (for sampling bags of grains, coffee beans, spices often referred to as “bag-thief” and other similar products stored in burlap bags). + Zone sampler (for sampling palm oil and similar products. A zone sampler is a sealed cylinder equipped with a value which opens automatically upon contact with the bottom of the tank or normally at any desired depth in the tank by means of an attached pull cord) + Hand towel/paper towel + Scientific Calculator + Disposable glove + String + Camera with zoom lens + Stapler . Official seal + Sealing wax + Official Label + Official Label Seal + Reftigerator (0-4°C) + Freezer (-18°C) + Coldbox (electrically operated with D.C. current, suitable for use in a vehicle). + Insulated containers (for transporting or holding chilled or frozen samples). + Writing materials — pen, maker, note pads, small/record book. A list of attire to be used during sampling for safety measures are as follows’ + Cap + Gloves + Helmet + Gloves (sterile) + Overall + Ear plug + Safety boots + Rain coat + Wellington boot + UV goggles + Mouth mask Note: The list of equipment is a general guide for food sampling activities. The individual re- quirement would vary with specific sampling activities to be carried out, for example, a zone sampler would be needed for sampling of palm oil and similar products. 23 42. ‘Sample containers ‘When selecting containers in which the samples are to be placed and kept, attention should be given in particular to the following general requirements: a) b) °) Cleanliness of the container (it may be necessary to specify special cleaning, drying, sterilizing, or other treatment, prior to filing with the sample). Quality of the containers, in particular: inertness, of all parts of the container, to the sample: suitability for withstanding, where appropriate, the various special treatments mentioned in a); robustness of the container to withstand hazards during the selected method of transport and, if a hazardous material is in the container, compliance with the regulations in force governing its transport, for example in the case of pressure vessels used as containers for the sample, the selection of suitably pressure-tested units; suitable for preserving the sample unchanged for the necessary period, for example by preventing any undesirable access of light, heat, or other radiation, and the passage of moisture or other gases or vapours into or out of the samples. choice of quality of the sample container to hold samples of a given material, depending on the use to which the sample is to be put; for example, while an air-tight container may be required for a sample for determining the volatile ‘matter content of the material, a plastic film bag may be adequate for a sample of the same material intended only for particle size analysis. Ullage (headspace) in the container after introducing the sample, including elimina- tion of headspace that might cause unfavourable change in the state of the sample (for example churning of cream). In, general, for liquids the authorised officer should use clean, dry containers of appropriate ‘waterproof and greaseproof material, including glass, stainless steel, and suitable plastic material which can be sterilized by heat if necessary. The containers must have a secure closure of rubber or plastic stoppers, or a screw-cap of metal or plastic, coated with an insoluble, non-absorbent and greaseproof material. The containers and closures must be such as not to influence the odour, flavour, pH, or composition of the sample products. For solids or semi-solids, clean, dry, wide-mouth, cylindrical recepticals of suitable waterproof, greaseproof material should be used. These containers may also need to be sterilized. All containers must have air-tight closures, Suitable plastics bags may also be used although plastic bags or containers should not be used for pesticide samples. SECTION 5. SAMPLING PROCEDURE 5A 52 524 5.2.2 Authorized Sampling Personnel In the context of the Food Regulations 1985, authorized sampling shall be authorised officers as defined under Section 3 of the Food Act 1983. Legal Procedure Food samples procured for enforcement purpose should comply with the procedure for taking samples for physical, chemical and microbiological analysis of food provided under Regulations 4 and 5 of the Food Regulations 1985 as in Sections 5.2.1. and 5.2.2. Procedure on taking samples for physical and chemical analysis ‘The authorised officer having procured a sample of food for the purpose of physical or chemical analysis should: a) mix liquid, free-flowing or suspended materials until the products is homogenous; ) divide the sample into three separate parts and mark and seal or fasten up each part in such a manner as its nature will permit; ©) offer one part to the seller, importer or manufacturer or his agent or the person ha- ving charge of the food; 4) deliver either personally or through another authorized officer or by A.R. (Ack- nowledgement of Receipt) registered mail one of the remaining parts to an analysis; and ¢) retain the other remaining part. Where a sample consist of any food contained in unopened packages and if in the opi- nion of the authorised officer the division of a sample for analysis into three separate parts is not reasonably practicable or might affect the composition or impede the pro- per analysis of the content, the authorised officer taking or otherwise procuring the sample should divide the package into the requisite number of lots and deals with each lotas if it were a part. However, if a particular package of food has or appears to have in it or upon in any fo- reign substance or any substance which is suspected of being poisonous, harmful or injurious to health; or itis not practicable to divide the sample into the requisite number of parts or lots, the authorised officer should take one sample without dividing it into separate parts and should subsequently deliver the sample so taken either personally or through another authorised officer or by A.R. (Acknowledgement of Receipt) registered ‘mail to an analyst Procedure on taking sample for microbiological analysis Where 2 sample of food is required for microbiological analysis, the authorized officer taking or otherwise procuring the sample should: 53 54 5.44 Part 1: Gyneral Principles And Procedure a) only take one sample and shall not divide such sample into separate parts; b) mark and seal the sample in such a manner as its nature will permits, and ©) deliver such sample personally or through another authorised officer to an analyst with the least practicable delay. Sampling for Monitoring Purpose For the purpose of monitoring and surveillance, samples should be taken according to procedures in Section 3 of this guidelines, Aseptic Sampling Aseptic sampling is a method used to obtain a sample of a product susceptible to microbiological contamination, such sample being collected without contaminating either the original lot or the sample being collected. Aseptic samples are collected and delivered to the analytical laboratory in a manner which will ensure that the microbiological findings accurately reflect the condition of the lot at the time of sampling. Products in large drums, or similar containers, either aseptically filled or heat processed, should not be sampled while the shipment is enroute unless there is an eminent danger to health and/or the owner accepts responsibility for the portion remaining in the sampled container. Sampling of these products should be undertaken at the consignee (user) so the remaining portion can be immediately used or stored under conditions ¢hat will maintain its bacteriological integrity after the sample is collected. ‘Whenever possible collect intact unopened containers for microbiological analysis. If it is necessary ¢0 open containers for sampling, draw the sample and submit it under conditions which will prevent multiplication or undue reduction of the bacterial population, Follow these basic principles of sampling for aseptic sampling; Use of sterilized equipment Use of sterilized equipment and containers These should be obtained from the laboratory. Equipment and containers sterilized by the laboratory must be properly taken care of to prevent contamination and properly stored if not used immediately. All pre-sterilized materials should be dated and identified by the laboratory and bear the name of the microbiologist who sterilized the equipment or containers, Some agencies purchase, one time use commercially pre-sterilized plastic container (whirl packs) that do not have to be re-sterilized by the laboratory. Pre-sterilized metal or plastic tools should be used. However, if pre-sterilized tools are not available, the metal ones can be sterilized immediately before use with a propane torch, spirit lamp or other safe flaming device. After flaming, permit the tool to cool in the air prior to using for sampling. Avoid contamination of the tool during cooling. This can be done either by preventing its contact with contaminated surfaces, or by cooling inside sterile container. Sometimes a hoot tool may be cooled in the product to be sampled, then moved to an untouched area for sampling. This procedure should be used with caution because the hot sampling tool may burn or otherwise affect the product. ob Parte General Principles And Procedure 5.4.2 55 Soaking the tool with 70% isopropanol and then flaming off is an acceptable method of field sterilization which may be used. (If there is a choice), dry heat sterilized implement from the laboratory should always be used, If it is necessary to sterilize in the field, the inspector should be extremely careful regarding the use of a propane torch or other flame when sterilizing tools and equipment. Evaluate the conditions pertaining to explosive vapours, dusty areas, flame restricted areas, and the firms policy before using flame, The use of stands or other supportive devices should be considered as the precaution when the torch is not being held in hand, Also, be sure that all fammable liquids, such as isopropanol, are in metals cans and not in breakable containers, If itis necessary to drill, saw, or cut items being sampled (such as large frozen fish, cheese wheels, frozen fruit, etc) use stainless steel bits, blades, knives, etc, if atall possible, Wooden handled sampling instruments are particularly susceptible to bacterial contamination, are difficult to sterilized, and should not be used. If itis necessary to handle the item being sampled, use sterilized tongs. For some sampling assignments sterile gloves (rubber, vinyl, plastic etc) are used but this method is not really practical because a fresh glove would have to be used for each sub-sample. Also an unused glove in a sterile container should be submitted as a control. Opening sterile sample containers Work rapidly, but carefully when collecting samples. Open sterile sampling containers only to admit the sample and close immediately after. Do not touch the inside of the sterile container, lip or lid. Do not allow the open lid te become contaminated. For each sample collected submit one container that has been opened and exposed to the air about the same amount of time as the container being sampled was open. This will serve as an open control which will provide information about the air-borne bacteria in the area where the sample was collected. Also submit with each sample collected a closed sterile container to serve as a closed control. The closed control is intended to show that the container in which the sample was collected was sterile and did not contribute to any microbiological contamination found in the sample. These controls along with the glove control previously mentioned should assure that any microbiological contamination found was in the sample and not contributed to by the inspector or the sampling implement. ‘Sampling in dusty areas Do not collect samples in areas where dust or atmospheric conditions may cause contamination of the sample, unless such contamination may be considered part of the sample. Example: the processing area may have a high level of dust present as a part of the operation and the product is exposed to these conditions. A sample collected under these condition would accurately reflect the normal situation to which the food is exposed. However, collection of an aseptic sample from a previously closed container in front of an open door with dust blowing in from the street would be exposing the product to abnormal conditions that may be reflected in the sample results. Packing, Sealing and Marking of Samples and Sample Containers 554 Filing and packing of sample and containres Samples collected in glass containers for later freezing should be transferred to expandable containers before freezing. If liquid must be frozen in glass, 77 5.52 DO NOT fill the container, leave sufficient room for the liquid to expand upon freezing otherwise the glass container may break. If possible, pre-cool the sample container. If freezer facilities are not available or if the sample is to be shipped, pack with dry ice in insulated cartons. DO NOT place dry ice inside of tightly closed metal, glass, plastic, or similar type containers that do not breathe. They may explode. If necessary to use this type of container adequately vent them to prevent built-up of excessive pressure. Conspicuously mark the other shipping cartons with the words “CONTAINS DRY ICE” When samples are in plastic type containers, the dry ice must be wrapped in paper to prevent direct contact with plastic. The extreme cold generated by the dry ice cause plastic to become brittle and may rupture thus losing the integrity of the sample, It is possible to keep the sample refrigerated and not frozen by using dry ice, however, to do so requires a good knowledge of the amount of dry ice to be used depending on the nature of the product and the amount of sample. Even if the proper amount of dry ice is used, the dry ice may freeze the edges of the product, so if itis imperative that no part of the sample becomes frozen, use coolants other than dry ice. In all packages where the inspector uses dry ice, it should be distributed as equally as possible on all sides of the sample package using pieces as small as possible to avoid “ hot spots” (Figure 2). The container should be insulated on all sides. All edges of the container should be taped to assist in the insulation Arrangement of Food Sample in a container: CORRECT WRONG Figure 2 Note: Procedures to obtain uniform distribution of ice and food sample in a container is illustrated in Appendix 8. Food samples must maintain a temperature of 0-5*C throughout in a refrigerator or an insulated cool container/cool box. Marking Labelling requirements Itis important that each sample should be unequivocally identifiable. To avoid any mistake, the sample or the container into which it is to be placed should be 28 Fart Ue General Principles Aad Procedure 5.5.24 given an identification marking immediately before or after the taking of the sample. Legal requirements Monitoring & Surveillance 5.5.2.2 55.2.3 For the purpose of enforcement as well as for monitoring and surveillance, label for food samples should comply with Regulation 6 of the Food Regulations 1985 as stated below: i) The label for food sample should be in duplicate with a common coun- terfoil in the form as prescribed in the second Schedule (Appendix 9). ii) Where a food sample is divide into three parts one of such label shall be pasted on each part of the sample while the remaining label is to be affixed with the request for analysis form. iii) In cases where only one food sample is taken only one of the label shall be pasted on such sample while another label is to be affixed to the request form. Identifying marks Each sample and sub-sample should be identified in a manner that can be related back to the lot from which it was sampled. The identification should also contain some distinctive mark that will indicate a month or even years later that a particular sample was indeed collected by him or her. The mark most commonly used for this purpose is the inspector’s initials. One way of identifying the subs in a sample is to assign a separate number to each sub. ‘When multiple subs are taken from cases, bales, boxes, etc, in a lot, arabic numerals and letters in combination may be used. For example: if 2 cans are taken from each case in the lot, the cans may be marked as sub number 1a, 1b, 2a, 2b, etc, to identify the subs as coming from case number 1, case number 2, ete, Other requirements. It is essential to emphasize that all labels should adhere firmly and that they and their marking should retain their function even when contaminated with the sample, and after exposure to the most severe conditions of storage of the sample that can reasonably be expected. Staples should not be used for micro- biological samples. If desirable, suitable protective coatings for the labels and marks may be specified. Any special requirements to be marked externally on the packed sample, for the information of the carriers, for example “fragile”, “keep cool”, “Keep refrigerated... °C”, “keep dry”, “store away from boilers” should be specified, Any requirements for cautionary markings, for example in the case of hazardous goods, should also be required to be conspicuously shown. 24 87 58 59 Packaging and Transmission of Laboratory Samples The sample to be sent to the laboratory must be placed in a clean inert container offering. adequate protection from external contamination and protection against damage to the sample in transit. The container must then be scaled in such a manner that unauthorised opening is detectable, and sent to the laboratory as soon as possible taking any necessary precautions against leakage or spoilage. For all chilled and frozen food, the ‘cold chain’ must be maintained A caution should be included that samples of incompatible materials which, if they were to come into contact, would constitute a hazard or otherwise have deleterious effects, for example cause a taint in the case of foodstuffs, should not be packed together in the same container. If it is necessary for sample to be shipped to the laboratory, the package must be secured with shock absorbing materials for protection from damage en route. Even ifthe original shipping container is used this does not assure that the sample will be safe. However, often some additional packing with crumpled newspaper will add that extra measure of protection that may be needed, Liquids or hard swelled cans will require more protection. Special precautions must also be taken when shipping products, in pressurized containers, to avoid possible exposure to excessive heat. Any shippers who use non-pressurized planes may also need this type of container to prevent explosion. Request For Analysis of Food Sample The request for analysis of food sample is provided under Regulation 7 of the Food Regulation 1985 as stated below: The request for analysis of food sample shall be made in Form A as set out in the Third Schedule (Appendix 10). ‘Sampling Report Asampling report for record purpose should be prepared, signed by the authorized officer collecting the samples. This report should be in the format as in Appendix 11. General Considerations Itis difficult to be specific about the handling ofa sample after itis collected. Requirements for the handling of samples and the parent lot of food from which the sample is collected may vary widely from country to country and for different purpose for which the sample was collected. The following information must therefore be considered as guidelines. Restoring lots sampled When collecting a sample from a whole sale or retail source, the authorised officer must try not to do anything that may jeopardize the dealers possibility of selling the remainder of the lot. If at all possible, especially when collecting a sample from a wholesaler, the authorised officer should not leave slack-filled shipping cases or short weight or short volume containers in the lot after sampling, Back filling is one method of assuring that the dealer has only full cases or merchandise left. Cases from which samples have been And Proce collected should be closed and glued shut, barrels and drums properly closed, bags resewn, ete. Identifying lots sampled Each shipping case from which a sample unit is collected should be identified in some distinctive way so the lot or any sampled container can be identified if necessary, such as the need to collect an additional sample or if the results of analysis are unfavourable and the remaining product should not be introduced into consumer channels. The identification should not be so conspicuous as to cause undue attention. Industrial or permanent type markers should not be used on containers subject to penetration. Penetration of some inks to the product may interfere with the planned analysis. If water base markers are used the identification should be covered with tape to prevent running,

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